User`s Manual - Department of Chemistry
Contents
1. 4 2 4 3 Touch Screen Main Page 4 2 4 4 Function Buttons 4 2 4 1 Introduction Operation Manual The glovebox system is operated through the touch screen All functions can be realized by touching the buttons on the touch screen 4 2 System Startup The switch for the main electric power supply to the glovebox is located on side of the electric control box The power is off when the switch is at 0 position and on when it is at 1 position 4 3 Touch Screen Main Page After powering up the system will perform self diagnosis The touch screen main page will appear in 30 seconds 2006 05 28 09 55 Box Press 2 53 mbar Oxygen 0 62 ppm Moisture 0 08 ppm Blower Purifier Vacuum 4 2 4 4 Function Buttons Operation Manual There are 11 function buttons on Main page All the function buttons will be explained in this section When the system encounters problems this button will flash Press the button to enter the Alarm page to get the information Touch this function button to enter the Auto evacuation page to set the auto evacuation parameters and start auto evacuation of large antechamber See Section 5 5 for details Touch this function button to enter the Circulation page2. 2 2 2 2 Connecting Box with Purifier Only for System with Stand alone Purifier 2 2 2 3 Connecting Gas Supply 2 2 2 4 Installing Gloves 2 3 2 5 Install Power Strip inside the BOX 2 4 2 6 Install Oxygen and Moisture Probe 2 6 2 1 g Or Operation Manual 2 1 Equipment Placement Four casters are installed on the stand of the equipment The equipment can be easily moved and position in the room After the positioning the glovebox at the desirable location please use a wrench to adjust the levelers at the four legs of the stand so that the casters are off the ground and the glovebox is leveled 2 2 Connecting the Box with the Purifier Only for the System with Stand alone Purifier 2 2 1 Connecting the circulation main pipe OD 1 2 2 2 Connecting the stainless tubing 3 8 2 3 Connecting Gases 2 3 1 Connecting the Working Gas Attach a gas regulator to a cylinder containing working gas which can high purity nitrogen or argon Using a piece of nylon tubing OD 8 mm maximum pressure 120 psi or copper tubing to connect the g
3. Increases capacity is near regeneration is the oxygen level returned depleted to lt I ppm Yes Problem fixed No Contact Vigor Service Dept Adsorbents may need replaced Oxygen Level Surges Leak at the Check the O ring on the antechamber when Antechamber door antechamber Are there any cracks on the O rings is open Yes Replace defect O rings No Take out O rings and grease them and reinstall them If the problem is not fixed contact Vigor Service Dept Frequent Regeneration 1 Air leaks into the Check the leak of the box Set the Required system pressure range to 5 to 10 mbar and 2 Damaged Adsorbent turn off the circulation system and waiting for 5 minutes for the system to stabilize before recording the oxygen level change with time for 2 hours If the leak rate is greater than 5 ppm hr there are leaks on the system If leak rate is less than 5 ppm hr the adsorbent needs replaced Operation Manual 6 7 Error Messages When Alarm is flashing the system is encountering some error and the messages are displayed on the Alarm page Press Alarm to enter the Alarm page Vacuum Overloaded The current Adjust the current dial on the switch allowed set too labeled 2 to higher amp low 2 Add more oil if oil is clear Oil level too low Change oil Oil too dirty Blower Overloaded Filter blocked Inspect the filter and change them if The current dirty allowed s
4. Vi l g Or Operation Manual 5 5 Antechamber Operations Antechamber is used to transfer materials into or out of the glovebox When transferring materials into the glovebox one need to perform a procedure to minimized the amount of the moisture and oxygen brought into the glovebox This procedure can be performed manually or automatically On the Main page of the touch screen there are two valves P lt connecting to the large antechamber The valve connecting the antechamber to a vacuum pump is used to evacuate the antechamber to remove air inside the antechamber space and on the surface of the materails The other connecting the antechamber to the box is used to refill the antechamber equalizing the pressure inside the antechamber with the atmospheric pressure so that the door on the antechamber can be opened Valve Status D lt Close P Open The status of the valve is changed between Close and Open by touching the valve on the touch screen Before opening the outside antechamber door make sure a The antechamber s inside door is closed b The refill valve is closed in solid blue c The antechamber is not under vacuum and the needle on the vacuum gauge should be at O position Always keep the antechamber under vacuum when not in use 5 11 5 5 1 Transferring Materials into Antechamber Operation Manual The following is a standard procedure to bring materials into the glovebox from air 1 Completel
5. rS is displayed and the system automatically loads the factory values and reboots in 5 seconds 2 4 Turn off on alarm When the buzzer sounds press AA to temporarily turn off buzzer If the problems are not fixed press AA again to restore the buzzer 2 5 Stored Freezer Temperatures 2 5 1 When the freezer temperature is equal or less than the set temperature for the first time the system actuates this function 2 5 2 Store the highest and lowest temperatures that the freezer has reached 2 5 3 Under normal state except E1 E2 EE press to show the highest temperature stored in the memory 2 5 4 When the highest temperature stored in the memory is shown press again to show the lowest registered temperature 2 5 5 Without pressing any button within 5 seconds the system return to display the freezer temperature 2 5 6 Press and hold for 3 seconds the current freezer temperature will be registered as the highest and lowest stored temperatures 2 5 7 The stored temperatures will not be erased because of power outage The data will be retrieved from memory when power is restored 3 Functions 3 1 Temperature Calibration Ot When thermocouple ages adjust this parameter to correct the temperature 3 2 Temperature Alarm When the freezer temperature is higher than AU or lower than AL the alarm goes off 3 3 Temperature Setting Protection To avoid the set temperature tS ou
6. parameter table for the abbreviations for all the parameters 2 1 1 To set tS to 35 C follow the procedure below 2 1 1 1 When tS is displayed press to show saved value 18 C as the factory preset valve 2 1 1 2 Press or A to AA adjust the value to a desired one for example 35 C 2 1 1 3 Press Set or wait 15 second to save the change 2 1 1 4 Press or A to AA select OU and then press Set or simply waiting for 15 seconds to exit the setting mode 2 1 2 Set all other parameters according to the procedure described above 2 1 3 Set tS under normal mode according to the following procedure 2 1 3 1 Press and hold for AA 3 second 18 C is shown Factory preset valve 2 1 3 2 Procedure to adjust the value is same as in 2 1 1 2 2 1 3 3 Press Set or wait for 5 seconds to save setting and exit the setting mode 2 2 Lock Setting 2 2 1 Press and hold AA for 3 seconds and the setting function is locked and LC is displayed When setting function is lock all parameter can t be adjusted 2 2 2 Press and hold AA again for 3 seconds the setting function is unlocked and UL is displayed When setting function is lock the parameters can be set 2 2 3 The setting lock is not affected by disruption of power supply The locking status will be retrieved from the memory after restoring power 2 3 Reload the factory preset valves Press AA and A at the same time and then supply the power
7. 3 3 3 5 Purifier Regeneration 3 4 3 6 Antechamber 3 5 3 1 Introduction Operation Manual The glovebox system is an enclosed system Aur leaks into the glovebox system through seals and gloves During the use oxygen and moisture are introduced into the glovebox when materials are taken into the box and cylinder gas is introduced into the box to maintain the pressure To maintain the oxygen and moisture level less than 1 ppm a gas purifier is attached to the box The purifier withdraws the contaminated gas from the glovebox and flow through the purifier to remove oxygen and moisture impurity The purified gas is then sent back to the box This purification circulation is used to maintain the impurity level in the box at desirable level The system has three functions purging circulation and regeneration They are described here in details but the operating procedure will in described in later chapters 3 2 Pressure Control The pressure inside the box is a relative pressure comparing to the surrounding atmospheric pressure A possible pressure indicates the pressure inside the box is greater than the outside atmospheric pressure while a negative pressure show a lower pressure inside the box The unit of the pressure used here is mbar or one thousandth of a bar The
8. 5 mbar 4 4 Vi Operation Manual Chapter 5 Operation Instructions 5 1 Purge 5 1 5 2 Circulation 5 3 5 3 Regeneration 5 6 5 4 System Settings 5 9 5 5 Antechamber 5 11 5 6 Chemistry Software 5 22 5 0 5 1 Purge Operation Manual When large amount of impurities are introduced into glovebox it is recommended that one immediately turn off the gas circulation system and purge the impurities out of the box Doing so can avoid introducing the impurities into the gas purification column and consume the purification capacity To activate the purge function the circulation system needs to be turned off See Section 5 2 for the details about how to turn off circulation On the Main page of the touch screen press and the following screen will appear Purge Settings Purging Time 30 min Elie A To start purge Main To return to Main page 5 1 A l g Or Operation M
9. 7 3 1 Of When the parameters are being set 4 Troubleshooting 4 1 Alarm Codes 4 1 1 UA indicates the freezer temperature gt AU UA and the freezer temperature are displayed alternatively 4 1 2 LA indicates the freezer temperature lt AL LA and the freezer temperature are displayed alternatively 4 1 3 tA indicates the board temperature gt 95 C tA is displayed 4 2 Troubleshooting Codes The compressor works according to Cr CS parameters When both Cr and CS are set to 0 the compressor will keep running 4 2 1 EE indicates memory abnormal If powering off and then on could not fix the problem send it to the manufacturer for repair 4 2 2 E1 indicates a faulty thermocouple Check the temperature and replace thermocouple 4 2 3 E2 indicates a faulty board temperature sensor send the manufacturer for repair 5 Parameter Table Functions tS td AU AL HS LS Ad AC Cr CS Ot Ft FC dL OU FOU mase Set freezer temperature Temperature Difference Upper alarm temperature Lower alarm temperature Upper set temperature Lower set temperature Alarm delay time Compressor delay time Resting time Temperature adjustment Fan stop running temperature Fan operation options Defrost temperature lock Value Ranges Upper UN p Nn AL 1 AN ee a D _ N Lower p lt pa fe 70
10. back into the box The continuous circulation will remove maintain the impurity level inside the box below desirable system Because the ultralow leak rate of Vigor gloveboxes the gas purification does not need to run continuously The auto circulation feature enable oxygen and moisture sensors to control the circulation system Typically the gas purification system works at only 10 of time and rests during 90 of the time 3 5 Purifier Regeneration The purifier column has limited capacities 60 L of O and 2 kg of H20 When oxygen or moisture level can t be maintained below the desirable value the purifier needs to be regenerated to recover the adsorption capacity The regeneration of the purifier need regeneration gas containing 5 reducing gas H2 The regeneration is done automatically according to the programs preloaded to the Programmable Logic Controller PLC on the system and the whole process will take 24 hours Warning Do not interrupt the regeneration program after it starts In case of 3 4 Operation Manual interruption of the regeneration process please do not restart the system Waiting overnight before starting the regeneration Contact Vigor service engineer for help 3 6 Antechamber Vigor glovebox box comes with a large antechamber ID 370 mm and a mini antechamber optional ID 100 mm or 150 mm The antechambers are used to transfer materials into out glovebox without introducing air into the
11. be immediately turned off and perform the purge until oxygen level decrease to below 100 ppm Some organic solvents may damage adsorbents When large amount of solvents is expected to be released into the box during an experiment it is recommended to turn off gas purifier to avoid admitting organic solvents into the purification column After completing the experiment purge the box for 5 minutes before turning on the purification system Leak through damaged gloves seals O2 gt 100 ppm Purge until O2 lt 100 ppm fittings a Large amount of solvents Purge 5 to 10 mintues Large amount of solvents spilled or l Large amount of solvents Purge 5 to 10 mintues released 3 4 Gas Purification System The glovebox system is not a leak free system Air continuously leaks into the box through rubber gloves flange fittings compression fittings and the interface of window box gloveport window glove gloveport To maintain the atmosphere inside the box continuously below 1 ppm a gas purification system is attached to the box as shown in the diagram below 3 3 Operation Manual Box Antechamber Purifier Adsorbents Blower The gas purification system typically contains a purifier column for removing impurities and a blower to assist the gas circulation The gas containing impurities is withdrawn into the gas purification system and pass through the purifier column to remove impurities The purified gas is discharged
12. gt F e N ey _ N 7 Factory Valve l p CO 45 40 25 30 _ Nn Nn Unit O O O O O O min min min min O O Note Compressor stop working at the temperature Compressor start working at tS td Set off alarm when the freezer temperature is equal to or higher than this value Alarm is set off once the freezer temperature reaches this value once Set of alarm when the freezer temperature is equal to or less than this value Alarm is set off once the freezer temperature reaches this value once The highest allowable temperature to be set The lowest allowable temperature to be set Buzzer delay time when the system set off alarm The compressor is delay by the set amount of time when the conditions to start the compressor is met Under EE and E1 the compressor working time When Cr 0 the compress stop working Under EE and E1 the compressor resting time When CS 0 the compress keeping working Freezer temperature correction Fan Stops working at this temperature 0 Working with the compressor 1 Continuous operation 0 Display the current temperature 1 Lock the freezer temperature when defrosting Exit the setting mode
13. opaque change the oil If the oil level is too low add more oil Can the pump start Yes Problem fixed No Go to next step Replace the breaker in for the vacuum pump Can the pump start Yes Problem fixed No Contact Vigor Service Dept Pump Oil loss 1 Gas blast is open Check to make sure the gas blast on the 2 Leak in the vacuum pump is close If it is open vacuum system close it Add more oil to raise the oil level close to the maximum line and check the oil level again one month lately No significant loss Problem fixed Significant loss Go to next step Check the vacuum line leakage Insert the vacuum pump vent line into water for 10 mintutes Without actuating the antechamber and box evacuation valve are there still gas continuously comes out of the vent line Yes Go to next step No No leak in the vacuum line Set the box working pressure range to 5 to 10 mbar After the box pressure reading stabilizes is the pressure Operation Manual continues decreasing at rate greater than 0 05mbar min Yes Contact Vigor Service Dept No No real from the box to the vacuum system Go to next step Tighten all the connections on the vacuum line Is there still gas coming out of the vent line Yes Contact Vigor Service Dept No Problem fixed 6 6 Problems with Oxygen Level inside the Box Oxygen Level Slowly The adsorption Regenerate the purifier After
14. this 5 3 YV l g Or Operation Manual Record Pressing this button to get to the circulation record page which shows the circulation data including total circulation time circulation time after last regeneration and the total regeneration number There are two circulation modes namely Auto and Manual The circulation mode is set by and pressing the circulation mode button which will change between Auto 5 2 1 Manual Circulation Set To stop the circulation at the manual mode press 5 2 2 Auto Circulation The circulation can also be set to Auto mode Under the Auto mode the circulation blower will start if the oxygen or moisture level is higher the O2 high or H2O high The blower will not stop until the oxygen and moisture are lower than O2 low and H2O low Operators can set O2 High O2 Low H2O High and H2O Low by pressing the value field Following is the procedure to set up the O2 High value 1 After pressing the field a key pad will appear on the touch screen 2 Input the desirable O2 High value which can have one digit after the decimal point 3 Press ENT key on the keypad Operation Manual 4 Repeat step 1 to 3 to set up O2 Low H2O High and H2O Low lt Note When the system powers on the circulation mode will be automatically set to Auto Mode and the impurity levels inside the box will be maintained below the set value Press to return to the main page
15. 3 55 to the field next to X1 7 Press Compute to calculate the molecular weight 5 24 A l g Or Operation Manual 8 Press Back register the molecular weight for the compound and return to Software page The formula can also be calculated using fragments of the molecule 1 Press clear to zero all fields next to the elements and groups 2 Enter 6 to the field next to element C 3 Enter 28 to the field next to element H 4 Enter 6 to the field next to element N 5 Enter 187 6 to the field next to X1 weight for Cu NO3 2 is 187 6 6 Press tof Compute calculate the molecular weight 7 Press Back register the molecular weight for the compound and return to Software page Note 1 Remember to zero all the field by pressing clear before entering formula Compute 2 After finishing entering formula remember to press to calculate the molecular weight 3 If the molecular weight for the compound is known just enter the weight to X1 and do not need to enter the formula 5 6 3 Calculating Chemical Reaction Input On Main page of the touch screen press to enter Software page where the chemical reaction input can be calculated The following is the procedure to calculate the input for a reaction to be performed 1 Enter the ratio of moles of the compounds in the chemical reaction stroicheometry below the compound A B C and D on the row leading by Sto 2 Calculate molecular weight for all compou
16. Glovebox amp Gas Purification System VG1200 750TS User s Manual Vigor Gas Separation Technologies Co Ltd Operation Manual Introduction Thank you for choosing Vigor s glovebox Please read this manual carefully before you install and use this equipment This manual will guide you to install and operate this equipment correctly If you have any question on this manual or have any problems about using this equipment please contact our service staff at 1 716 200 1200 Please do not make copies of this manual to a third party without obtaining a written permit from Vigor This manual is only for operators of this glovebox and Vigor s service staff Thank you again for selecting our glovebox and we hope you will enjoy using our equipment and Edition 08 2006 l Operation Manual Chapter 1 Preparation 1 1 Location Preparation 1 1 1 2 Gas Supply 1 1 1 3 Power Supply 1 2 1 1 Location Preparation Operation Manual 1 1 1 Room Room Temperature Minimum 15 C 50 F Maximum 30 C 86 F Humidity 20 to 70 Good Ventilation 1 1 2 Floor Flat Strong enough to support the weight of the equipment 1 2 Gas Supply
17. Press to enter the Circulation Record page Circulation Record Circ Time after last Regen E hr Total regen No os The Circulation Record page displays the total circulation time circulation time after last regeneration and the total number of regeneration These data show the status of the purifier and are useful for maintenance and repair of the equipment 5 5 5 3 Purifier Regeneration Operation Manual Stop the circulation before activate the regeneration process On the main page press JR em to enter the Purifier Regeneration page Purifier Regeneration EUN Start Regeneration Regeneration time Left 1440 min Adjust Regen Gas Flow AANE GAIEN To start adjusting regeneration gas flow A Adju J just Regen Gas Flow To stop adjusting regeneration gas flow Stop Regeneration To stop regeneration ESS To pause the regeneration process Continue To continue the regeneration program 5 6 A l g Or Operation Manual 5 3 1 Regeneration gas The adsorption of oxygen by the purifier is an irreversible chemical adsorption process Therefore the regeneration of the purifier requires a reducing gas A gas mixture containing about 5 of hydrogen balanced by the working gas is recommended If you working gas is argon use a gas mixture containing 5 or hydrogen and 95 of argon If your working gas is nitrogen use a hydrogen nitrogen 5 95 mixture At least half cyl
18. Working Gas Purpose Required for operating the equipment Used to create an inert atmosphere inside the box Used to operating the pneumatic valves Type of the Gas Nitrogen Argon or Helium To support a uninterrupted gas supply Cylinder Cylinder Regulator for Type K cylinders with 3000 psi regulating to at least Regulators 70 psi Compression Fittings Provided by the manufacturer Regeneration Gas Used to regenerate the adsorbents in Type T purifier when the purifier is Purposes saturated with the impurity gases Type of Gas Depending on the type of the working gas used for the glovebox system a When nitrogen is used as the working gas please use nitrogen hydrogen mixture 95 N 5 H b When argon is used as the working gas please use nitrogen hydrogen mixture 95 Ar 5 H When helium is used as the working gas please use helium hydrogen mixture 95 He 5 H l 1 Operation Manual Quantity Each regeneration requires half to one full cylinder Type K Regulator Cylinder Regulators for Type K cylinders with 3000 psi regulating to 30 psi Connections Compression Fittings 1 3 Power Supply This equipment use single phase 110V 60 Hz electric power The power rating depends on the model of the product Please see the product information plate for the current required by the equipment g Or Operation Manual Chapter 2 Installation 2 1 Placement of the Glovebox
19. anual After the purge function is activated the system will introduce working gas into the box to increase the box pressure before opening the box vent valve The system will continue introducing the working gas to purge the impurities out of the box for the amount of time set by the operator The purge action can be terminated at any time The following is the purging procedure 1 Set the purging time in minutes Press the data field area and a keyboard will appear Enter the a desirable value as the purging time 2 Press to activate the purging function After activating the purging function the button will become 3 The program will automatically stop after the purging time expires The button will 4 The purging program can be stopped at any time and the button will become to stop purging 5 2 5 2 Circulation Operation Manual Before starting circulation please make sure a The box is not being purged b The purifier is not being regenerated Don t start circulation if the box is being purged or the purifier is being regenerated On the main page press Circ the following screen will appear Purifier Circulation Settings Circulation Mode Ea Auto Circulation Oy High a ppm Settings O2 Low ppm H20 High ppm H20 Low ppm Circulation mode Auto At this mode the blower and the circulation will be automatically controlled by the Auto Circulation settings After pressing it
20. as regulator to the working gas port on the glovebox Adjust the regulator to deliver the working gas at 4 to 5 bar 65 to 75 psi lt Warning Setting the pressure too high will damage the equipment but the glovebox will not work properly if the pressure is too low 2 3 2 Connecting the Regeneration Gas Attach a gas regulator to cylinder containing the regeneration gas Using a piece of 3 8 plastic tubing maximum pressure 120 psi or copper tubing to connect the gas regulator to the working gas port on the glovebox Adjust the regulator to deliver the regeneration gas at 1 bar 15 psi lt gt Warning Too high pressure may damage the equipment 2 3 3 Vent During the regeneration of the purifier the regeneration gas flows through the heated purifier to the vent port Because the purifier adsorbs some chemicals and the regeneration gas contains hydrogen the gas coming out of the purifier may contain chemicals as well as un reacted hydrogen Therefore it should be vented to outdoor or to a fume hood lt Precaution The exhausted gas from the regeneration may contain un reacted hydrogen and harmful chemicals It could have unpleasant odors and pollute the lab and may harm the equipment operators It is recommended to vent the exhorted gas directly to outdoor or to a fume hood 2 2 g Or Operation Manual Warning If harmful materials are used in the glovebox all the exhausted gas from the glovebox system including the reg
21. box To transfer materials into the box first open the outer door of the antechamber refill the antechamber if it is under vacuum Place the materials in the slide tray inside the antechamber and then close the outer door Evacuate the air inside the antechamber for 20 to 30 minutes and refill the antechamber halfway so that the vacuum gauge on the antechamber is around 0 5 bar Repeat the evacuation refill process two more times to minimize the amount of the impurities be taken into the box Fully refill the antechamber and open the inner door and transfer materials into the box Close the inner door and evacuate the antechamber To transfer the materials out of the box first evacuate the antechamber and fully refill the antechamber Open the inner door and transfer materials into the antechamber Close the inner door and open the outer door to transfer materials out of the antechamber Close the outer door and evacuate the antechamber Warning Do not try to open the antechamber doors while the antechamber is under vacuum Forcefully open the door will damage the equipment lt Caution Do not open the outer and inner door simultaneously Make sure there is no air in the antechamber before opening the inner door 3 5 Chapter 4 System Startup Operation Manual 4 1 Introduction 4 2 4 2 Startup
22. de antechamber door 6 Turn the door clockwise into the slot 5 20 Operation Manual 7 Turn the door handle clockwise to tighten the door 8 Turn the three way valve beneath Mini Antechamber to Evacuation position to evacuation air out of the antechamber The needle on the vacuum gauge move to 1 0 direction Evacuate 5 minutes for no porous materials overnight for porous materials such as paper If possible heat porous materials in the oven for several hours before transferring into Mini antechamber 9 Refill Mini Antechamber by turning the three way valve to Refill position 10 Repeat Step 8 and 9 two more times 11 Completely refill Mini Antechamber so that the needle on the vacuum gauge at O position 12 Turn the three way valve to Close position 13 Use left hand to open Mini Antechamber inner door 14 Pull the tray out of the antechamber and remove materials from the tray and place them in the box 15 If there are any materials to be transferred out of box through Mini Antechamber place them into the tray 16 Put the tray back into the antechamber 17 Close the antechamber door 18 Open the outside antechamber door IMPORTANT Make sure the three way valve is at Close position 19 Take out the tray and remove the materials from the tray 20 Close the antechamber door 21 Evacuate the antechamber Note Always keep the antechamber under vacuum when not in use 5 21 5 6 Chemical Software Opera
23. eneration purging and vacuum pump should be vented directly to outdoor or a functioning fume hood 2 3 4 Vacuum Pump Exhausted Gas Vent the exhausted gas from the vacuum pump to outdoor or a functioning fume hood 2 4 Install Gloves 1 Insert you hand and arm into the glove to be installed and slide glove into the box through the glove port Rotate the glove so that the thumb is pointed up 2 Slide your hand out and turn the cuff inside out and over the gloveport Rotate the cuff of the glove to further adjust the thumb s position if needed 3 There are three grooves on the glove port Adjust the glove cuff so that the rim of the glove is position in the first groove from the window Place two O rings over the gloves and on the other two grooves 4 Repeat steps above to install all other gloves 2 3 g Or Operation Manual 2 5 Install Power Strip inside the Glovebox There are four spare KF40 Flange fittings which could be used for feedthroughs for electric power electric signals gas liquid and vacuum A power strip with a Flange fitting is provided The following is a installation procedure 1 If the box is still an air box skip this step To avoid introducing air into the box adjust the pressure inside the box to at least 5 mbar by setting the lower limit of the box pressure to Smbar 2 Remove a blanking Flange on a feedthrough you choose to use for the power supply 3 Feed the
24. ervice and the equipment Department No Replace valves Operation Manual 6 4 Circulation Problems Turn on the switch for the blower in the Press 1 Current Overload but the circulation did again Observe whether the switch not start and the system y break again displays warning Yes Go to next step message Blower gt No Problem fixed abnormal Check whether the circulation path is blocked Yes Clean the circulation path No Go to next step After replacing the switch does the switch breaks again Yes Contact Vigor Service Dept No Go to next step The pressure of Set working gas pressure to 4 5 bar Press but the circulation 70 80 psi and press Does system show the working gas 1s did not start and the the same warning message l too low warning message display FCHZ1 no feedback or 2 Solenoid valve FCHZ2 no feedback malfunction Yes Go to next step No Problem fixed Check whether the relay switches and Circulation valve solenoid valves work properly malfunction Yes Go to next step No Replace defect parts Replace the circulation valves Does system show the same warning message Yes Contact Vigor Service Dept No Problems fixed Operation Manual 6 5 Vacuum Problems Vacuum pump cannot 1 Current overload Check the pump oil If the oil is dirty start 2 Overheat brown color or
25. et too Adjust the current dial on switch 1 toa low higher amp FCHZI no feedback or Working gas 1 Set the working gas pressure to 75 psi FCHZ2 no feedback pressure is too Fix the feedback switch on the valve low The faulty feedback switch on the valve on the purifier O2 exceeds the set Oxygen Inspect the box and take correcting actions valve concentration in the to bring the oxygen concentration within the box exceeds the set allowable range value H2O exceeds the set Moisture Inspect the box and take correcting actions valve concentration in the to bring the moisture concentration within box exceeds the set the allowable range value Freezer Operation Instruction 1 Specifications 1 1 Extenal Dimensions 550mm H x 400mm W x300mm D 1 2 Internal Dimensions 450mm H x 300mm W x 220mm D 1 3 Operation Environment 5 to 55 C or 23 to 131 F lt 90 RH 1 4 Power Supply AC 110 410 single phase 50 60Hz 1 5 Power consumption 300W 1 6 Freezer Temperature Range 40 C 70 C Error 1 C 1 7 Input Output 1 7 1 Temperature Sensor NTC 1 5 m L x 2 1 7 2 Compressors Output Contacts Capacity 16 5 A 120VAC 1 7 3 Fan Contact Capacity 8 3 A 120VAC 1 7 4 Alarm Output Internal buzzer 2 Operating Instructions 2 1 Setting Mode Press and hold for 3 seconds to enter setting mode and tS is displayed Press Al or BA to select a different parameter to adjust See the
26. formed by the program The default number is 3 Evacuation Time The duration of each evacuation excluding last evacuation to be performed 5 16 A l g Or Operation Manual The default value is 30 mintues Last Evacuation The duration of last evacuation The default value is 30 mintues The following is the auto evacuation procedure 1 Enter the number of evacuation refill cycles The number of cycles is usually set to 3 2 Enter the time in minutes for each evacuation 3 Enter the time in minutes for last evacuation 4 Press to start the auto evacuation program 5 The auto evacuation program will perform the action based on the parameters entered by the operator 6 The program can be stop anytime by pressing on Stop Antechamber Auto Evacuation page 5 17 Vi l g Or Operation Manual 5 5 4 Transferring Materials into Box After the evacuation refill procedure is completed the materials are ready to be transferred from the antechamber into the box following the procedure below 1 Turn on the refill valve by press icon on Main screen Wait until the vacuum gauge on antechamber reach 0 2 Close the refill valve IMPORTANT Do not forget to close the refill valve 3 Open the inner door of the antechamber 4 Pull out the sliding tray and remove the materials from the sliding tray and place them in the box 5 Put anything to be removed from the box into the sliding tray 6 Push the sliding
27. ftware page press the blue field on MW line below compound A B C and D to enter Molecular Weight Calculation page Users are prompted to enter the formula for the corresponding compound The program will calculate the molecular weight and return the value to the field There are three buttons on the page clear To zero all the field on this page Compute To calculate the molecular weight based on the formula entered Back To return to the Software page and enter the molecular weight to the field On this page there are 12 frequently used elements C H N O F Cl Br I Li Na K Ca and 4 groups X1 X2 X3 X4 The elements form 3 columns and the groups is located on the th 4 column The field next to an element is for the number of the atom present in the formula while the field next to a group is for weight of the group The group can be an organic functional groups such as C4H9 elements such Fe or part of a molecule such as FeCl and Cu NO3 2 Compound Cu NH2CH2CH2NH2 3 NO3 2 or C6H28N8O6Cu is used here as an example to show how to calculate the molecular weight There is more than one way to do the calculation One can use formula to perform the calculation 1 Press clear to zero all fields next to the elements and groups 2 Enter 6 to the field next to element C 3 Enter 28 to the field next to element H 4 Enter 8 to the field next to element N 5 Enter 6 to the field next to element O 6 Enter 6
28. ge is about 0 5 and press evacuation valve to stop refill and start evacuation 4 Repeat evacuation refill two more times 5 Last refill allow the pressures inside the antechamber and the box totally equalized indicating by the needle on the gauge reach 0 6 Close the refill valve to cut of connection between the antechamber and the box to avoid accidentally admitting air into the box when the antechamber outside door is opened 5 5 3 Auto Evacuation Refill 5 15 Transferring materials into the box through the large antechamber is a time consuming process and requires operator s attention Even the user remembers to refill the antechamber every 20 to 30 minutes the whole process usually required more than 90 minutes It is difficult Operation Manual to perform the refill on time resulting much longer time may be needed to finish the process To increase the efficiency and save user s time an auto evacuation refill function have been added to the system On Main page of the touch screen press PAIESE to enter the Antechamber Auto Evacuation page Antechamber Auto Evacuation oe No of Evac Refill zs Evacuation Time a min Last Evacuation Ea min To start auto evacuation process Default To set the default values as the parameters Main To return to Main page No of Evac Refill This value field host a positive whole number the number of the evacuation refill cycles to be per
29. generation After finish adjusting the regeneration gas flow press to start regeneration The preloaded programs on the PLC will automatically perform various actions including heating the purifier evacuating the purifier passing regeneration gas and cooling the purifier The regeneration will take 24 hours to finish During the regeneration Regen button will keep flashing until the regeneration program 5 7 ends Operation Manual During the regeneration the program can be paused To pause the regeneration program press _ The program can be resume by pressing press Stop Regeneration After pressing this button a new window will appear and the user will be prompted to choose to stop or continue the regeneration program Cancel Regeneration Process To Stop the regeneration To continue the regeneration its To return to the Purifier Regeneration page P l To go to the Main page 5 8 5 4 System Settings Operation Manual There are many parameters can be set for the system However some parameters are for the users to set while others are for the service technicians On the Mian page users can enter the System Settings page by pressing System Settings Box Pressure Upper Ex mbar Lower Ea mbar Alarm O2 Limit 10 ppm H20 Limit EA ppm Default Load the default value into the field next to the button Expert Settings To enter the Expert Settings page T
30. he expert settings include system system settings such as regeneration parameters and are for service technicians only Main To return to the Main page Vi l g Or Operation Manual 5 4 1 Set Box Pressure The box working pressure can be control by the PLC Users can define the working pressure range and the system will adjust the pressure within the set range at all time To set the upper and lower limit of the working pressure press Settings to get to the System Settings page Touch the field for the Upper and a keypad will appear Enter a desirable value and press the ENTER key Do the same to the field for the lower limit of the box pressure Note The minimum rage of the working pressure should be set to 2 mbar It is Alarm recommend to set the upper limit to 3 mbar and the lower limit to O or 1 Vigor gloveboxes with patented seal technologies have very low leak rate even at negative box pressure To ease sweating set the pressure the negative so that gloves will wrap your hands and arms giving better ventilation 5 4 2 Set Impurity Alarm Level Users can also set the oxygen and moisture alarm levels To set the alarm level touch the field for the alarm limits and a keypad will appear Enter a desirable value and pressure ENTER key on the keypad When either impurity level exceeds the set value the alarm will be triggered to inform users On the Main page Settings button will start flashing 5 10
31. inder of gas is required for the regeneration Install a regulator on the gas cylinder the pressure inside the cylinder should be greater than 1100 psi or 70 bar Set the output pressure to 15 psi or 1 bar 5 3 2 Adjust Regeneration Gas Flow Before starting regeneration of the purifier please stop the circulation see the Section 5 2 During the regeneration the purifier is first heated and evacuated for 3 hours and then the regeneration gas is passed through the purifier for 3 hours Please set the following rate so that when the regeneration gas will be introduced to the purifier at the right flow rate Occasional attention is recommended during the reduction of the purifier Check the flow rate and vent from time to time and make sure the gas is enough to last three hours based on the consumption rate The following is the precdure to adjust the regeneration gas flow a Turn on the cylinder valve and make sure the cylinder pressure is greater than 1100 psi or 70 bar b Set the cylinder regulator pressure to 15 psig or 1 bar c On Main page of the touch screen press Circ to enter the Circulation page to stop the gas circulation see Section 5 2 for details d On Main page press to go to the Purifier Regeneration page e Press RNGhiNmiouomerke aloes on the Purifier Regeneration page f Wait until the gas flow out of the regeneration vent and adjust the flow rate to 4 line on the flow meter g Press 5 3 3 Start Re
32. lation on the filter please change the filter Quartly to avoid damaging the blower Change oil after regeneration or once a year whichever come first Anually Operation Manual Antechamber Check antechamber O rings annually If there are any signs of Annually O Rings deterioration of material of the O ring replace it Operation Manual 6 3 Purge Problems Gas circulation is in Turn off the gas circulation seeing pre Start Pern but the function did not start progress Section 5 2 for details 2 Run out of working 2 Change a new gas cylinder gas Sten Purging 1 Did the valve get electric signal Press Purge vent valve did not Veen Replace thie valve but pressure inside open Go to next step the box surged 2 Check whether the relay switch for the valve working properly Yes Contact Vigor Service Department No Replace the replay switch star Purging 1 Replace the gas cylinder Press No working gas l Turn on the working gas the box pressure Working gas is not decreased rapidly and Set the pressure to 2 bar opened oxygen concentration Check the tubing connections for leak jump Delivery pressure Check whether valve get electric signal for working pressure Yes Replace valves is too low No Go to next step Air leaks on the Check whether the relay switch for the tubing connecting valve works properly working gas source Yes Contact Vigor S
33. lculation Main To return to Main page A B C and D represent compounds involved in the chemical reaction Those four compounds can be reactants or products The reaction can be one of the following n A gt n B n C n D n A n B gt n C n D n A n B n C gt nf D n A n B n C nf D gt Stoi stands for Stoichiometry The coefficients in the balanced chemical reactions above nf n n and n should be enter in the corresponding field in the row MW stands for Molecular Weight Touching the field in the row will take the user to the Molecular Weight Calculation page More details about how to calculate molecular weight will be presented later in this section Wt stands for Weight the amount needed for the chemical reaction When the calculation base is set to w weight for compound A is entered at the first field in the row in green the weight of compound of B C and D are automatically calculated and shown in the corresponding fields in white 5 23 A l g Or Operation Manual mmol stands for milimoles the number of the milimoles needed for the chemical reaction When the calculation base is set to mmol the number for compound A is entered at the first field in the row in green the weight of all compounds A B C and D are automatically calculated and shown in the fields 5 6 2 Molecular Weight Calculation On the Chemical So
34. nds by pressing the blue fields See Section 6 5 2 for more details 3 Set the calculation base which can be w or mmol 4 Enter the weight of mmol for Compound A a Enter the weight for Compund A at the designated field when the calculation base is set to w b Enter the mmol for Compound A at the designated field when the calculation base 5 The input or theoretical yield for all other compounds are calculated Note If a solution with known molar concentration to be used use the calculated input in milimoles to calculate the volume required for the reaction 5 25 Chapter 6 Maintenance and Troubleshooting Operation Manual 6 1 Introduction 6 1 6 2 Maintenances 6 1 6 3 Purging Problems 6 3 6 4 Circulation Problems 6 4 6 5 Vacuum Problems 6 5 6 6 Oxygen Problem 6 6 6 7 Error Message 6 7 6 0 6 1 I
35. ntroduction Operation Manual The glovebox system is designed to run without too much maintenance However some simple maintenance is required The system software can also detect problems and show the information to help operator to fix the problems This chapter will also provide information about troubleshooting of the system 6 2 Maintenance The system requires some simple maintenance See the following table for details Check working gas cylinder to make there is enough gas to perform Working Gas the task Stock one cylinder to avoid interruption of use of the Daily glovebox Check to make sure the gloves are in good condition and there is no holes on them Set the box pressure to gt 5 mbar and wait for a Glove couple of minutes for pressure to stabilize If the pressure Daily continue to drop at rate greater than 0 02 mbar minute the box may leaks and probably through the gloves When the solvent adsorber is saturated organic vapor will start to Solvent accumulate inside the box If strong odors come out of the Adsorber antechamber it is time to change the adsorbents in the solvent a adsorber Check the pump oil color and level New pump oil is almost clear Pump Oil liquid When it turns brown the oil should be changed If the oil Monthly Level level is approaching the minimum level add additional oil into the z pump Check the filters at the inlet and outlet of the purification system Filter If a visible dust accumu
36. plug that will be used to attach the power strip through the KF40 O ring 4 Slide the power cable into the box until the Flange on the 2 4 g Or Operation Manual cable reach the KF40 Oring on the flange on the box Use a KF40 clamp to attach two Flanges and tighten it 5 Place the power strip into the box through a glove port or antechamber 6 Connect the power plug on the power strip to the plug on the flange 2 6 Install Oxygen and Moisture Analyzers Fuel cell oxygen sensor is very sensitive to air To avoid prolong exposure to high oxygen level in air the sensor is sealed under nitrogen until it is ready to install to a glovebox with low oxygen concentration Therefore oxygen sensor is installed only when the oxygen level inside the box is lower than 100 ppm 2 6 1 Moisture Analyzer Please see the user s manual of moisture analyzer 2 6 2 Oxygen Analyzer Please see the User s Manual of Oxygen Analyzer 2 5 Operation Manual Chapter 3 Working Principles 3 1 Introduction 3 1 3 2 Pressure Control 3 1 3 3 Purging the BOX 3 2 3 4 Gas Purification
37. pressure of the box is controlled by the PLC The user sets the upper and lower limits of the pressure on the touch screen interface and the PLC will regulate the pressure to within the set limits The pressure can be set to either positive or negative min min max max 2mbar 10mbar 10mbar 12mbar Highest Working Highest Box Lowest Box Pressure Pressure Pressure The working pressure in the box can be controlled to a pressure ranging from 10 mbar to 10 mbar To The range of the working pressure can be set so the control system will automatically maintain the working pressure within the set range Users set the upper and lower limits of the range of the working pressure 3 1 Highest Box Pressure The highest pressure allowed in the box is 12 mbar When the box Operation Manual pressure higher than 12 the safety valve on the glovebox is actuated to vent the excess pressure to avoid damage to the equipment Lowest Box Pressure The lowest pressure of the glovebox in the box is 12 mbar When the box pressure is lower than 12 mbar the glovebox will be shut down Upper Set Point The box pressure is regulated lower than the Upper Set Point When the box pressure is higher than the set point the valve connecting the box and the vacuum system is opened and the gas inside the box is evacuated to lower the box pressure lower than the set point Lower Set Point The box pressure is reg
38. side is closed the air in the antechamber can be evacuated by a vacuum pump For non porous materials the residual pressure in antechamber can be pump down to 10 bar in 10 minutes To minimize the amount of impurities taken into the box it is recommended to evacuate the antechamber for 20 to 30 minutes each time For porous materials the evacuation time should be much longer It could be several hours to several days It is recommended to heat the materials in the oven to remove majority of the moisture and move hot materials into the antechamber right before the evacuation The following is the evacuation refill precedure 1 Close the antechamber ourside door 2 On the Main page of the touch screen press icon representing the evacuation valve which connects the antechamber to the vacuum pump When the valve is turned on the icon will change from solid blue into yellow filled and an animated gas flow from antechamber to the vacuum pump indicates the evacuation is in progress 3 After evacuated for 20 to 30 minutes press the icon representing the refill valve which connects the antechamber to the box to refill the antechamber After the icon is pressed the refill valve is turned on while the evacuation valve is automatically closed because the program only allow one of the two to be open at any time An animated gas flow from the box to the antechamber indicating the refill is in progress Refill the antechamber until the vacuum gau
39. t of the capability of the compressor set HS and LS to limit the temperature range for tS 3 4 Board Temperature Protection At When the board temperature 95 C the controller turns off the compressor switch and display flashing tA and set off alarm The tA alarm will not be clear until the temperature reaches 75 or below 3 5 Compress Operation 3 5 1 When the freezer temperature reaches the set temperature tS compressor stop working When the freezer temperature rises to the set temperature tS plus the set temperature difference td the compressor is restarted 3 5 2 Compressor Delay Start The delay time can be set by adjusting the parameter AC When the system requires turning on the compressor it starts the countdown and the compressor will not start until the countdown reach the delay time The start of compressor is delayed by one minute every time when the freezer is turned on 3 6 Power Outage Protection When power outage occurs during use the system will reloaded the parameters and continues operations after the power is restored 3 7 Light Signals 3 7 1 Comp Compressor Light 3 7 1 1 Steady On When the compress is working 3 7 1 2 Flashing When the compressor is in delay countdown mode 3 7 1 3 Off When the compress is off or the parameters are being adjusted 3 7 2 Defr Defrosting Signal Light Omitted 3 7 3 Fan Fan Signal Light 3 7 3 1 Steady on When Fan is working 3
40. tion Manual The system comes with chemical software as an optional feature The software package contains programs to calculate molecular weight from chemical formula amounts of chemicals needed for a given chemical reaction theoretical yields the reaction yield It also contains a simple calculator The software package enables users to do the calculations on the touch screen 5 6 1 Chemical Software Page Press Software to enter Software page Software PA Calculation base At this mode the calculations will be done based on weight Users enter a value of the weight required for compound A in the field at the first column and third row the weight required for all other chemicals will be calculated When wt is pressed it become mmol mmol Calculation base At this mode the calculations will be done based on milimoles Users enter a number of milimoles in the field at the first column and fourth row the 5 22 A l g Or Operation Manual weight required for all other chemicals will be calculated When is mmol pressed it w become Fields for entering values such as stoicheometry weight or number of milimoles Touch the field and the user will be prompted to enter a value Fields for calculating molecular weight Touch the field and the user will be brought to Molecular Weight Calculation page Displays calculation results Calculator Calculator to perform arithmetic ca
41. to control the purifier circulation See Section 5 2 for more details Touch this function key to turn on the box light Touch again to turn the light off Touch this function key to enter the Purging page to set purging time and perform purge of the box This function is disabled while the gas circulation is in progress See Section 5 1 for details Touch this function button to enter the Purifier Regeneration page See Section 5 3 for more details Note The purifier regeneration process will start while the circulation is in process See Section 5 3 for details Touch this function key to enter the System Settings page where the system parameters are entered The system parameters enter here include the box pressure limits and alarm setting off limits of impurities See Section 5 4 for details Touch this function button to enter the Software page where the chemistry related calculations are performed See Section 5 6 for details 4 3 Operation Manual This function icon represents a valve Itis solid blue when it is close Touch the button will turn on the valve When the valve is open the button change to gt lt gt lt This icon represents the vacuum pump on the glovebox system Touch the icon will turn on the vacuum pump and touch it again to turn it off When the pump is on the cross inside the circle turns It stops while the ier vacuum pump is off This icon display the box pressure and the range is 5 to
42. tray back into the antechamber 7 Close the antechamber door 8 Open the outside door to remove anything to be brought out of box IMPORTANT Make sure that refill valve is close When the refill valve and outside door are both open the box is connected to the air and air may be admitted into the box 9 Evacuate the antechamber by pressing the evacuation valve on Main page Note It isa good practice to keep antechamber under vacuum when not in use 5 18 5 5 5 Mini Antechamber Operation Operation Manual Mini antechamber is used to transfer small volume of materials Because the volume of the mini antechamber is much smaller than the large antechamber it takes much less time to evacuate it In addition it take consume much less inert gas during the process Take the same precautions as transferring materials through the large antechamber Before opening the ourside door on the mini antechamber make sure a The antechamber s inside door is closed b The three way valve is at Close position c The antechamber is not under vacuum and the needle on the vacuum gauge should be at 0 position 1 Turn the handle on the outside door counterclockwise until the door is loose 2 Turn the door counterclockwise 5 19 Operation Manual 3 Remove the door from the antechamber 4 Put materials to be transferred into the box in the removable tray slide back the tray into the mini antechamber 5 Put up the outsi
43. ulated higher than the Lower Set Point When the box pressure is lower than the set point the valve connecting the box and the gas supply system is opened and the gas from the supply system is added into the box to raise the box pressure over the lower set point Highest Working Pressure The highest pressure can be set as 10 mbar Lowest Working Pressure The lowest working pressure is 10 mbar 3 3 Purge Impurities inside the glovebox are removed by gas purification system However the purifier has limited capacities When the concentrations of the impurities are too high it is not recommended to use the purifier remove them In stead a process called purging is used to quickly remove large amount of impurities from the box The purging process quickly passes large amount of high purity nitrogen through the box to flush the impurity out of the box Purge can be done either manually or automatically When a new box is installed the initial atmosphere is air and required to be purged before turning on the gas circulation system When air is admitted into the box due to inappropriate operations the oxygen may rise to over 100 ppm One should be immediately stop the purification system and purge the box to below 50 ppm before turning the purification system back on 3 2 Operation Manual When gloves or seals are damaged air may leak into the box and raise impurity level to gt 100 ppm The purification system should
44. y refill the antechamber and then close refill valve Before opening antechamber door make sure Needle on the vacuum gauge is at 0 Inner antechamber door is closed Refill valve is closed solid blue on the touch screen 2 Turn the handle on the antechamber door counterclockwise to open the door 3 Raise the bar on the door 5 12 4 The air spring will raise the door above the opening of the antechamber 5 Pull out the sliding tray 6 Place the materials on the sliding tray For easy access from inside the box place materials as far inside the antechamber as possible Operation Manual 5 13 Operation Manual 7 Push the sliding tray back into the antechamber 8 Pull the bar on the door down until it reach the rest post 9 Use fingers to turn the door handle clockwise to push the door touch the O ring on the antechamber and then turn another quarter of a turn 5 5 2 Manual Evacuation Refil After the materials are placed into the antechamber the antechamber is filled with air The Operation Manual gas impurities oxygen and moisture exist in two forms namely the gaseous form in the antechamber space and adsorbed form on the surface and pores of the materials to be taken into the glovebox Itis easier to remove the gaseous impurities than the adsorbed impurities To remove the air in the antechamber and on the materials a standard evacuation refill procedure is used After the out
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